HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 86661850, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 58081198 | HCID 58081198 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86661850 | HCID 86661850 | — |
Reaction Steps
To a mixture of tert-butyl 5-cyano-4,6-dimethylpyridin-2-ylcarbamate (10.8 g, 43.7 mmol) in THF (100 ml) were added about 15 cm3 of a Raney-Ni suspension in MeOH under Ar. The flask was sealed, and the suspension was vigorously stirred at it for 6 d under an atmosphere of hydrogen. The reaction mixture was filtered over a plug of cellite and eluted with DCM (200 ml), DCM-MeOH (9:1, 200 ml) and NH3 in MeOH (7N, 100 ml). Removal of all volatiles in vacuo afforded the crude product which was recrystallized from MeOH-DCM to afford the title compound. LCMS RtM=1.13 min, [M+H]+=252.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09290485B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-13f93e086b254b80b5f5e4c0448aa482 |
| Source note | uspto-grants-2016_03 |